The third generation (G‐3) polypropylenimine hexadecaamine dendrimer (DAB‐Am‐16) was grafted onto the silica gel surface. The modified silica interacts easily with Cu2+ and then with potassium ferrocyanide to form copper hexacyanoferrate. The modified silica was characterized by the following techniques: Nuclear Magnetic Resonance (NMR), FTIR spectroscopy, Energy Dispersive X‐ray (EDX) and Cyclic Voltammetry. The modified silica containing copper hexacyanoferrate (CuHCFSD) was tested for a voltammetric determination of nitrite using a modified graphite paste electrode.

The present work describes the preparation of nanoparticles of copper pentacyanonitrosyl complexes starting from the compound sodium nitroprusside. Copper pentacyanonitrosylferrate (NCuNP) nanoparticles were successfully synthesized by using deionized water and formamide as solvent. The material was characterized by Fourier-transforming infrared spectroscopy (FT-IR), X-ray diffraction (XRD), ultraviolet-visible (UV-Vis) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and cyclic voltammetry (CV). The results revealed that the electronic spectra of NCuNP exhibited a broad intervalence charge transfer band at 685 nm. An XRD peak broadening pattern of the NCuNP was verified, indicating a particle decrease when formamide is used. The particle size of NCuNP is estimated to be 80 nm. The cyclic voltammogram of the modified graphite paste electrode with NCuNP showed two redox pairs with formal potentialsEθ′=0.36 V andEθ′=0.78 V (ν=20 mV s−1; KCl 1.0 M), attributed to the redox processCuI/CuIIand [FeII(CN)5NO]/[FeIII(CN)5NO], respectively. The graphite paste electrode with NCuNP presents electrocatalytic response for Sulfite determination.

The octakis(3-chloropropyl)silsesquioxane (SS) was organofunctionalized with 4-amino-5-4(pyridyl)-4H-1,2,4-triazole-3-thiol. The product formed (SA) was undergo another reactions in two steps, first with copper and so hexacyanoferrate (III) to form CuHSA. The organofunctionalized silsesquioxane was characterized by the following techniques: scanning electron microscopy (SEM), Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR) in solid state, and thermogravimetric analysis in air and nitrogen atmosphere. The composite CuHSA was incorporated into a graphite paste electrode and the electrochemical behavior studies were conducted with cyclic voltammetry. The cyclic voltammogram of the modified graphite paste electrode with CuHSA showed one redox couple with formal potentialEθ′=0.75 V versus Ag/AgCl(sat)(KCl 1.0 mol L−1;v= 20 mV s−1) attributed to the redox process Fe(II)(CN)6/Fe(III)(CN)6of the binuclear complex formed. The redox couple presents an electrocatalytic response of sulfhydryl compounds such as n-acetylcysteine and l-cysteine. For determination of n-acetylcysteine and l-cysteine the modified graphite paste electrode showed a linear region in the concentration range of 2 to 20 mmol L−1. The modified electrode was chemically and electrochemically stable and showed good reproducibility.

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